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Method and equipment for preparing ethyl triphenyl phosphonium bromide

A technology of triphenylethylphosphonium bromide and triphenylphosphonium bromide, which is applied in the field of preparation of triphenylethylphosphonium bromide, can solve problems such as unspecified preparation methods, achieve increased reaction effect, increase reaction rate, The effect of increasing contact

Inactive Publication Date: 2019-01-04
JIANGXI KENTE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Including by weight: 47-50 parts of bisphenol F / resorcinol copolymerized epoxy resin, 10-15 parts of silicone modified epoxy resin, 3-5 parts of butyl ether benzomelamine resin, methyl 15-16 parts of acrylic acid, 14-18 parts of acrylic acid, 6-8 parts of fumaric acid, 9-15 parts of maleic anhydride, 0.5-1 part of triphenylethylphosphonium bromide, 0.3-0.6 parts of hydroquinone 45-48 parts of styrene, 0.2-0.5 parts of photoinitiator, 2-5 parts of reactive diluent, 0.3-0.8 parts of photoinitiating compounding agent, 5-8 parts of composite modifier, and the two documents give the triphenyl ethylphosphonium bromide as the raw material of the invention, but did not give the corresponding preparation method
[0003] There is no preparation method of triphenylethylphosphonium bromide in the existing literature, so the present invention further researches and prepares its preparation method

Method used

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  • Method and equipment for preparing ethyl triphenyl phosphonium bromide

Examples

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Comparison scheme
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Embodiment 1

[0021] see figure 1 , a kind of method for preparing triphenylethylphosphonium bromide of the present embodiment, comprises the following steps:

[0022] Step 1, pretreatment: place bromoethane at a temperature of 20°C, let it stand for 45 minutes, and then perform microwave treatment.

[0023] Then place the triphenylphosphonium at 30°C for 25 minutes, and set aside;

[0024] Step 2, add bromoethane and triphenylphosphonium in step 1 to absolute ethanol according to the weight ratio of 2:1, then send them into the reaction kettle, the reaction temperature is 90°C, react for 20min, and then add bromo Benzene, continue to react for 1 hour, then raise the temperature to 160°C and keep it warm for 20 minutes to obtain the triphenylethylphosphonium bromide of the present invention.

[0025] The microwave treatment conditions of this embodiment are: microwave frequency 300MHz, power 700-W, microwave treatment method is microwave treatment 35s and then stop for 1min, then microwav...

Embodiment 2

[0030] A kind of method for preparing triphenylethylphosphonium bromide of the present embodiment, comprises the following steps:

[0031] Step 1, pretreatment: place bromoethane at a temperature of 30°C, let it stand for 55 minutes, and then perform microwave treatment.

[0032] Then place the triphenylphosphonium at 40°C for 35 minutes, and set aside;

[0033] Step 2, add bromoethane and triphenylphosphonium in step 1 to absolute ethanol according to the weight ratio of 2:1, then send them into the reaction kettle, the reaction temperature is 110°C, react for 30min, and then add bromo Benzene, continue to react for 2 hours, then raise the temperature to 170°C and keep it warm for 30 minutes to obtain the triphenylethylphosphonium bromide of the present invention.

[0034] The microwave treatment conditions of this embodiment are: microwave frequency 400MHz, power 780W, microwave treatment method is 45s after microwave treatment, stop for 2min, then stop for 55s after microw...

Embodiment 3

[0039] A kind of method for preparing triphenylethylphosphonium bromide of the present embodiment, comprises the following steps:

[0040] Step 1, pretreatment: place bromoethane at a temperature of 25°C, let it stand for 50 minutes, and then perform microwave treatment.

[0041] Then, place the triphenylphosphonium at 35°C for 30 minutes, and set aside;

[0042] Step 2, add bromoethane and triphenylphosphonium in step 1 to absolute ethanol according to the weight ratio of 2:1, then send them into the reaction kettle, the reaction temperature is 100°C, react for 25min, and then add bromo Benzene, continue to react for 1.5h, then raise the temperature to 165°C and keep it warm for 25min to obtain the triphenylethylphosphonium bromide of the present invention.

[0043] The microwave treatment conditions of this embodiment are: microwave frequency 350MHz, power 740W, microwave treatment method is 40s after microwave treatment, then stop for 1.5min, then microwave treatment for 2...

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Abstract

The invention relates to the technical field of preparation of ethyl triphenyl phosphonium bromide, in particular to a method and equipment for preparing ethyl triphenyl phosphonium bromide. The method comprises the following steps: 1, performing pretreatment: placing bromoethane at the temperature of 20 to 30 DEG C, standing for 45 to 55 minutes, performing microwave treatment, placing triphenylphosphonium at the temperature of 30 to 40 DEG C, and standing for 25 to 35 minutes for future use; and 2, adding the bromoethane and the triphenyl phosphonium in the step 1 into absolute ethanol according to the weight ratio of 2:1 and then feeding into a reaction kettle. The bromoethane is pretreated, so that the contact degree of the bromoethane and the triphenyl phosphoniumis increased and thereaction effect is improved; then the materials are added into the reaction kettle to perform mixed reaction, so that the yield and the purity are obviously improved; and through the mutual proportion and pretreatment of the raw materials, the reaction rate and the reaction yield are greatly improved compared with those in the prior art.

Description

technical field [0001] The invention relates to the technical field of preparing triphenylethylphosphonium bromide, in particular to a method and equipment for preparing triphenylethylphosphonium bromide. Background technique [0002] Triphenylethylphosphonium bromide, also known as ethyltriphenylphosphonium bromide, has the molecular formula C h BrP, with a molecular weight of 371.2506, is irritating to the eyes, respiratory system and skin. The existing Chinese patent document (publication number: CN106832795A) discloses a high-temperature-resistant and anti-corrosion vinyl resin, which includes: bisphenol A formaldehyde ring 33-36 parts of oxygen resin, 10-12 parts of silicone modified epoxy resin, 2-4 parts of acrylic acid modified alkyd resin, 15-16 parts of methacrylic acid, 10-13 parts of acrylic acid, 11 parts of fumaric acid -14 parts, 15-18 parts of maleic anhydride, 0.5-1 part of triphenylethylphosphonium bromide, 0.2-0.5 parts of hydroquinone, 40-43 parts of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/54
CPCC07F9/5442
Inventor 张朵龙健朝刘宇
Owner JIANGXI KENTE CHEM CO LTD